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Tetrabutylammonium Fluoride → 4-Chloro-1-ethynyl-2-fluorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 反応物 | ((4-Chloro-2-fluorophenyl)ethynyl)trimethylsilane | HCID 90019293 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Chloro-1-ethynyl-2-fluorobenzene | HCID 50998794 | 73.2% |
反応手順
To a solution of ((4-chloro-2-fluorophenyl)ethynyl)trimethylsilane (1.0 g, 4.42 mmol) in DCM (20 mL) was added TBAF (catalytic) and reaction mixture was stirred for 1-2 h at RT. The reaction mass was quenched in water, extracted with DCM and concentrated to afford 0.900 g of the crude product which was further purified by column chromatography eluting with pet. ether to afford to afford 0.500 g of pure product. 1H NMR (300 MHz, DMSO d6): δ 4.60 (s, 1H), 7.32 (d, J=8.1 Hz, 1H), 7.56-7.61 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-c89a7419ef5c4f178e8a5c1eb06a8e57 |
| 出典メモ | uspto-grants-2016_09 |